CN104725142B - A kind of chitosan coated material of adjustable sustained release performance and preparation method thereof - Google Patents
A kind of chitosan coated material of adjustable sustained release performance and preparation method thereof Download PDFInfo
- Publication number
- CN104725142B CN104725142B CN201510132579.1A CN201510132579A CN104725142B CN 104725142 B CN104725142 B CN 104725142B CN 201510132579 A CN201510132579 A CN 201510132579A CN 104725142 B CN104725142 B CN 104725142B
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- CN
- China
- Prior art keywords
- chitosan
- blocked isocyanate
- crosslinking agent
- ketene dimer
- sustained release
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Classifications
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G5/00—Fertilisers characterised by their form
- C05G5/30—Layered or coated, e.g. dust-preventing coatings
- C05G5/37—Layered or coated, e.g. dust-preventing coatings layered or coated with a polymer
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- Life Sciences & Earth Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Fertilizers (AREA)
Abstract
The present invention discloses a kind of chitosan coated material of adjustable sustained release performance and preparation method thereof, it is that chitosan is modified by alkyl ketene dimer to obtain hydrophobic chitosan slow-release material, alkyl ketene dimer is reacted with hydroxyl active in chitosan chain, amino so that long-chain hydrophobic group is introduced in chitosan chain.Blocked isocyanate crosslinking agent and modified obtained chitosan derivatives are prepared by mixing into release-controlled coated solution.The grafting rate of chitosan is different, and the hydrophobic ability of chitosan derivatives is different, and how much dosage of crosslinking agent can change the crosslinking degree of material, the sustained release performance of coated fertilizer is adjusted with this, reach the target of suitable different crops growth cycle needs.
Description
Technical field
The invention belongs to fertilizer slow release coating field, be related to a kind of adjustable sustained release performance chitosan coated material and its
Preparation method.
Background technology
Nowadays the organic coated material category used in fertilizer slow release coating is more, and organic coated material has polymer
(vistanex, polyethylene, polystyrene, alkyd resin etc.), tar, rubber, latex, paraffin, pitch, oils etc., this
The sustained release performance that a little organic materials are difficult to adjust fertilizer can not be degraded again, and soil environment can be polluted.
Chitosan has very abundant biological source, is biodegradable material.Medicine, table can be widely used in
The fields such as face activating agent, separation material.Due to there is the presence of a large amount of amino and hydroxyl on chitosan chain, hydrophilic ability is stronger, right
The sustained release performance of fertilizer is poor, can chemically change its hydrophilic and hydrophobic in structure.Further expand the application of chitosan.
The content of the invention
In view of the shortcomings of the prior art, the present invention proposes a kind of chitosan coated material and its system of adjustable sustained release performance
Preparation Method.
Chitosan relative molecular weight used is 50~700,000 in the present invention, and deacetylation is 80~100%.
Chitosan and alkyl ketene dimer react in the present invention is carried out in suitable organic solvent, solvent be toluene,
The mass ratio of one kind in chloroform, dichloroethanes, chitosan and solvent is 1：20.
In the present invention, chitosan is scattered in organic solvent, adds alkyl ketene dimer and base catalyst, chitosan
It is 4 with alkyl ketene dimer mass ratio：1~1：5, base catalyst is the 1%~3% of chitosan mass, is warming up to 70~120
DEG C, 4~8h is reacted, separation is dried to obtain the chitosan derivatives of hydrophobically modified.By blocked isocyanate crosslinking agent and chitosan
Derivative, which is dissolved in the dilute acetic acid solution that mass fraction is 2~4%, is prepared into release-controlled coated liquid, and chitosan derivatives are different with blocking
The mass ratio of cyanate is 20：1~10：1, blocked isocyanate crosslinking agent is 2~3 degrees of functionality, and deblocking temperature is 90~120
DEG C, the mass ratio of chitosan derivatives and dilute acetic acid solution is 1：50~2：25.
In the present invention, chitosan and alkyl ketene dimer reaction, chain hydrophobic side base is introduced.But chitosan is not still up to
To the requirement of fertilizer slow release coating, blocked isocyanate is added, the isocyanates that heating solution is honored as a queen makes chitosan crosslinked, enters one
The sustained release performance of step section material, can reach the requirement of fertilizer slow release coating.Release-controlled coated material preparation process in the present invention
Simply.The mass ratio of regulation chitosan and alkyl ketene dimer adjusts the grafting rate of chitosan, adjusts chitosan derivatives
Adjust the crosslinking degree of material with the mass ratio of blocked isocyanate, sustained release performance can by adjust the grafting rate of chitosan with
And crosslinking degree regulates and controls, it can meet that different crops grow needs, and such release-controlled coated material belongs to degradation material, can
To reduce the pollution to soil environment, the utilization rate of fertilizer is improved.
Embodiment
With reference to way of example, the present invention is described in further detail.
Embodiment one
The modification of step 1. chitosan：6g chitosans are scattered in toluene solvant, and are stirred until homogeneous, add butyl alkene
Ketone dimer 5g, 0.06g sodium hydroxide, reaction is warming up to 70 DEG C, reacts 4h.Reaction end separation is dried to obtain chitosan and spread out
Biology.
2g chitosan derivatives and 0.17g blocked isocyanates are dissolved in 100g2% dilute acetic acid solution by step 2., obtain
To release-controlled coated liquid.
Embodiment two
6g chitosans are scattered in chloroform solvent by step 1., and are stirred until homogeneous, and add dodecylene ketone dimer
10g, 0.12g sodium hydroxide, 90 DEG C are warming up to, react 5h.Separation is dried to obtain chitosan derivatives after reaction terminates.
2g chitosan derivatives and 0.15g blocked isocyanates are dissolved in 100g2% dilute acetic acid solution by step 2., obtain
To release-controlled coated liquid.
Embodiment three
6g chitosans are scattered in toluene solvant by step 1., and are stirred until homogeneous, and add tetradecene ketone dimer
12g, 0.18g potassium hydroxide, 100 DEG C are warming up to, react 6h.Reaction terminates separation and is dried to obtain chitosan derivatives.
2g chitosan derivatives and 0.13g blocked isocyanates are dissolved in 100g2% dilute acetic acid solution by step 2., obtain
To release-controlled coated liquid.
Example IV
6g chitosans are scattered in toluene solvant by step 1., and are stirred until homogeneous, and add hexadecene ketone dimer
14g, 0.18g sodium hydroxide, 110 DEG C are warming up to, react 6h.Separation is dried to obtain chitosan derivatives after reaction terminates.
2g chitosan derivatives and 0.1g blocked isocyanates are dissolved in 100g2% dilute acetic acid solution by step 2., are delayed
Release coating liquid.
Claims (5)
1. a kind of preparation method of the chitosan coated material of adjustable sustained release performance, is that chitosan is scattered in into organic solvent
In, alkyl ketene dimer and base catalyst are added, for a period of time, separation is dried to obtain the shell of hydrophobically modified to heating heating response
Polysaccharid derivative, chitosan derivatives and blocked isocyanate crosslinking agent are mixed to be dissolved in dilute acetic acid solution being prepared into be sustained and wrapped
Film liquid；The molecular weight of chitosan is 50~700,000, and deacetylation is 80~100%；Reaction is in toluene, chloroform, dichloromethane
Carried out in a kind of organic solvent therein, the mass ratio of chitosan and solvent is 1：20；Chitosan and alkyl ketene dimer matter
Amount is than being 4：1~1：5；The blocked isocyanate crosslinking agent used is 2~3 degrees of functionality, and it is 90~120 DEG C to unseal temperature, shell
The mass ratio of glycan and blocked isocyanate is 20：1~10：1.
2. according to the method described in claim 1, it is characterised in that the general structure of alkyl ketene dimer is：
Wherein, R, R ' for the alkyl chain of 4~16 carbon.
3. according to the method described in claim 1, it is characterised in that the temperature of reaction be 70~120 DEG C, the reaction time be 4~
8h。
4. according to the method described in claim 1, it is characterised in that the base catalyst of addition is the 1%~3% of chitosan mass,
Wherein base catalyst is one kind in sodium hydroxide, potassium hydroxide.
5. according to the method described in claim 1, it is characterised in that chitosan derivatives and blocked isocyanate crosslinking agent are dissolved in
Mass fraction is in 2~4% dilute acetic acid solution, and the mass ratio of chitosan derivatives and spirit of vinegar is 1：50~2：25.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510132579.1A CN104725142B (en) | 2015-03-25 | 2015-03-25 | A kind of chitosan coated material of adjustable sustained release performance and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510132579.1A CN104725142B (en) | 2015-03-25 | 2015-03-25 | A kind of chitosan coated material of adjustable sustained release performance and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN104725142A CN104725142A (en) | 2015-06-24 |
| CN104725142B true CN104725142B (en) | 2017-12-19 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510132579.1A Expired - Fee Related CN104725142B (en) | 2015-03-25 | 2015-03-25 | A kind of chitosan coated material of adjustable sustained release performance and preparation method thereof |
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| Country | Link |
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| CN (1) | CN104725142B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107793228A (en) * | 2017-11-21 | 2018-03-13 | 常州创索新材料科技有限公司 | A kind of preparation method of the hydrophobic coated fertilizer of biodegradation type |
| CN111484373A (en) * | 2020-06-11 | 2020-08-04 | 福建师范大学 | Preparation method of slow-release fertilizer coating liquid using alkyl ketene dimer |
| CN114181015B (en) * | 2021-12-30 | 2022-11-15 | 中农金瑞肥业有限公司 | Composite slow-release compound fertilizer special for wheat and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1621455A (en) * | 2004-10-14 | 2005-06-01 | 武汉理工大学 | Method for preparing hydrophobic inorganic and organic composite corpuscle |
| CN101631838A (en) * | 2007-02-19 | 2010-01-20 | 西洛芬股份公司 | The polymeric film or the coating that comprise hemicellulose |
| CN101942780A (en) * | 2010-09-15 | 2011-01-12 | 山东轻工业学院 | Method for preparing AKD emulsion sizing agent |
-
2015
- 2015-03-25 CN CN201510132579.1A patent/CN104725142B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1621455A (en) * | 2004-10-14 | 2005-06-01 | 武汉理工大学 | Method for preparing hydrophobic inorganic and organic composite corpuscle |
| CN101631838A (en) * | 2007-02-19 | 2010-01-20 | 西洛芬股份公司 | The polymeric film or the coating that comprise hemicellulose |
| CN101942780A (en) * | 2010-09-15 | 2011-01-12 | 山东轻工业学院 | Method for preparing AKD emulsion sizing agent |
Non-Patent Citations (3)
| Title |
|---|
| 可生物降解的壳聚糖肥料包膜材料的研究;陈强等;《高分子材料科学与工程》;20050528;第21卷(第3期);290-293 * |
| 新型生物降解交联剂的制备和交联壳聚糖的性能;杨媛等;《材料研究学报》;20070125;第21卷(第1期);25-31 * |
| 烷基烯酮二聚体改性瓜尔胶的制备及应用;薛贝等;《中国造纸》;20110915;第30卷(第9期);23-27 * |
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Granted publication date: 20171219 Termination date: 20210325 |